oldguy Posted April 10, 2011 Posted April 10, 2011 (edited) Anyone know of an inexpensive source for say 10 ++ lbs.I found some on ebay, but at $35 per Kilo, plus shipping.That seems high. EDIT TO ADD:After a lot of searching, it appears one can make a crystalline cellulose powder fairly comparable to store bought Microcrystalline Cellulose (MCC) by boiling cotton in a 10% HCI solution for 2 hours. Giving about an 80% yield of fine powder once dried. Any opinions if that is true ? Edited April 10, 2011 by oldguy
NightHawkInLight Posted April 10, 2011 Posted April 10, 2011 After a lot of searching, it appears one can make a crystalline cellulose powder fairly comparable to store bought Microcrystalline Cellulose (MCC) by boiling cotton in a 10% HCI solution for 2 hours. Giving about an 80% yield of fine powder once dried. Any opinions if that is true ? If that's true I would be very interested myself. I was looking for some about a year ago but after asking around discovered that it's hard to come by cheaply, not because it's expensive to manufacture, but because almost all the primary uses are industrial and the suppliers don't want to deal in small (<1000 or so lb) sales. Now that I think about it, what on earth did I want it for...I think I wanted to try to make nitrocellulose based color stars or something.
Mumbles Posted April 11, 2011 Posted April 11, 2011 I often heard NaOH to get pure crystalline cellulose, but I bet either would work as the key step is hydrolysis. It does work, but it probably wont be as consistent as a commercial products. Then again for what we need it for, that isn't so critical. MCNC (microcrystalline nitrocellulose) stars are pretty and clean burning, but require large amounts of NC base and some rather exotic colorants/reagents.
oldguy Posted November 8, 2011 Author Posted November 8, 2011 (edited) http://home.kpn.nl/v...k/Cellulose.pdf You can gleam a kitchen safe method for making MCC in small amounts from the link above.Not hard to ramp up the process for producing larger amounts of MCC either. Edited November 11, 2011 by oldguy
NightHawkInLight Posted November 9, 2011 Posted November 9, 2011 http://home.kpn.nl/vheeswijk/Cellulose.pdf You can gleam a kitchen safe method for making MCC in small amounts from the link above.Not hard to ramp up the process for producing larger amounts of MCC either. Nice find! I'm not sure how I feel about filling my oven with HCl vapor, maybe the toaster oven...Definitely something I'll look into further.
oldguy Posted November 9, 2011 Author Posted November 9, 2011 Nice find! I'm not sure how I feel about filling my oven with HCl vapor, maybe the toaster oven...Definitely something I'll look into further. OVEN.....? Stove top or a hot plate outside.
Mumbles Posted November 9, 2011 Posted November 9, 2011 Off the top of my head, the process may not require heating, just longer reaction times. I bet a good soaking for a few days may do the trick quite well.
PersonGuyDude Posted November 9, 2011 Posted November 9, 2011 What would you use Microcrystalline Cellulose for?Maybe nitration? Primes?
optimus Posted November 9, 2011 Posted November 9, 2011 MCNC (microcrystalline nitrocellulose) stars are pretty and clean burning, but require large amounts of NC base and some rather exotic colorants/reagents. I never really heard much about these stars - any chance of some further info?
NightHawkInLight Posted November 9, 2011 Posted November 9, 2011 OVEN.....? Stove top or a hot plate outside. That's what they mention was used.
oldguy Posted November 9, 2011 Author Posted November 9, 2011 (edited) What would you use Microcrystalline Cellulose for?Maybe nitration? Primes? For nitration. By itself Microcrystalline cellulose (MCC) is used as a dry binder for about every pill or tablet pharmaceutical companies make. Some time ago, I was fortunate enough to acquire some microcrystalline nitrocellulose (MCNC). It has a bulk density far higher than normal nitrocellulose (NC). Hence, burns much hotter than NC. It is easy to ignite and burns off near smokeless. MCNC will compact dry with minimal pressure (think simple arbor press, or a rotary tablet press) into a very hard durable plastic like mass. Since no water, alcohol, acetone, etc is required, generally there are no incompatibility issues with solvents or reactive metals. Edited November 11, 2011 by oldguy
oldguy Posted November 9, 2011 Author Posted November 9, 2011 I never really heard much about these stars - any chance of some further info? A good read on MCNC stars, etc.http://www.freepatentsonline.com/y2007/0068610.html
oldguy Posted November 10, 2011 Author Posted November 10, 2011 Statement: Microcrystalline cellulose (MCC) is prepared by hydrolyzing waste cotton fabric with 2.5 N hydrochloric acid at 100°C for 30 min. Question: 2.5 N = what percent?
Adrenaline Posted November 10, 2011 Posted November 10, 2011 N(Hcl)= 36.46 g/mol c(HCl)= 2.5mol/l --->m(HCl)= 2.5mol*36.46g/mol = 91,15g--->c(HCl)=91,15g /1000g=0,09115 = ~ 9,1 %
Mumbles Posted November 11, 2011 Posted November 11, 2011 One small correction if you don't mind. Moles per liter implies moles per volume. Moles per kilogram is Molality. 1L of HCl weights more than 1000g though. 2.5M is closer to 7.5%. Concentrated HCl (37%) is about 12.1M.
oldguy Posted November 12, 2011 Author Posted November 12, 2011 (edited) Tried this outdoors today with direct heat from a lab hot plate, using very heavy duty ¼ inch thick Pyrex (percolator type) coffee pot & lid as a boiling flask .Used (roughly) 10% HCI & (roughly) 105 to 110C temp for a little over an hour. I didn't weigh the cotton used at the start, but just eyeballing the finished batch, MCC yield appears around 75 to 80%. Edited November 12, 2011 by oldguy
asilentbob Posted November 12, 2011 Posted November 12, 2011 (edited) Just started a below room temperature attempt using a cut up cotton shirt and eyeballed addition of pool grade HCl. Just put it in a beaker, covered with saran and secured with a rubber band. Then the beaker was placed into a plastic bucket just in case of any very unlikely catastrophic failure. I'm not in a hurry. Edit: Left it for ~20h slightly below room temp with whatever concentration HCl it must have been, maybe 5-10%. Then had some free time so heated it up to between 45-90 C or so on and off for many many hours loosing a bunch of water. Then I added some more pool grade HCl to the beaker and kept up the temperatures for a while. After a while the fabric just starts to fall apart and a glass stir rod can push through the layers with just a little resistance... For me around this point bumping started to be a concern. I had wayyy too much cotton shirt (all of it) in the 800ml beaker which actually started out being filled with fluid + shirt up to ~900ml. So I reduced the temperature and tried to stir somewhat frequently. Many hours later a large part of the contents is powder with a bunch of small pieces of visibly woven cloth. I didn't inspect my cotton shirt very well, part of it was obviously not cotton, perhaps the threaded parts were nylon or some other synthetic. These parts fell off the rest and I had to fish out as much as I could from the bottom of the beaker. A few more times stirring it over several hours and now I have turned off the hot plate. I may let it sit for some hours as I still see some large particulate floating around... large as in on close inspection the woven pattern is still visible. I'll decant as much acid as I can, then transfer to a large Erlenmeyer flask to wash and decant a few more times. So basically if your going to destroy an entire shirt, for easier stirring and less bumping you probably want something like 1.5L volume of reaction and some boiling chips. Cutting up the shirt into small pieces and using a overhead stirrer could be useful, but the cloth may just get stuck on the stirrer. The concentration and temperature can speed up the reaction, but I think you could do it without, over a much longer time. Like a month maybe. Edited November 13, 2011 by asilentbob
oldguy Posted November 13, 2011 Author Posted November 13, 2011 (edited) Even though they say they are "cotton" on the label. Cotton T shirts are not always 100% cotton material. Some are blends of polyester and cotton. All the seams are usually sewn with some type of synthetic thread, usually polyester blends. Light a small piece on fire. Polyester blends will burn very quickly, leaving a plastic-like residue behind.Cotton will burn slowly, like a candle wick with an ash residue. Blends feel slick, almost silky, 100% cotton doesn't. Blends will not hold a crease, cotton will. I know it's "ghetto" but I simply bust up a ceramic plate into small pieces about 4 mesh.Then add some to the flask as (throw away) boiling chips to help prevent bumping. Edited November 14, 2011 by oldguy
asilentbob Posted November 18, 2011 Posted November 18, 2011 Its sitting in a beaker under water that has been decanted and re-filled several times to decrease the acidity somewhat. The vast majority of it is wayyyy too small to filter out, it would just pass through and some would clog the filter. I would like to keep it relatively free from sodium contamination, but I don't have any potassium carbonate / hydroxide, so it may just sit until I eventually get some. I know that you can get semi-bulk sodium carbonate for pools, can you find potassium carbonate for that too? Maybe a hydroponics store? Hmm...
Mumbles Posted November 18, 2011 Posted November 18, 2011 I eventually broke down and bought some K2CO3 from a soap making supply store. I've heard it can be found in certain fertilizers as potash. When I tried to actually go that route, I found they labeled pretty much every potassium based fertilizer as potash indiscriminately. I found both KCl and K2SO4 that way, as well as potassium phosphate under a different name.
oldguy Posted November 19, 2011 Author Posted November 19, 2011 (edited) Its sitting in a beaker under water that has been decanted and re-filled several times to decrease the acidity somewhat. The vast majority of it is wayyyy too small to filter out, it would just pass through and some would clog the filter. I would like to keep it relatively free from sodium contamination, but I don't have any potassium carbonate / hydroxide, so it may just sit until I eventually get some. I know that you can get semi-bulk sodium carbonate for pools, can you find potassium carbonate for that too? Maybe a hydroponics store? Hmm... http://www.ebay.com/itm/Potassium-Carbonate-5-Pounds-/150654517194?pt=LH_DefaultDomain_0&hash=item2313b57fca http://www.soapgoods...nate-p-719.html Edited November 19, 2011 by oldguy
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